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1 5 5 Vol. 5 No Journal of Food Safety and Quality May., 2014 * 刘慧玲 (, ) 摘要 :,,,,,,,,,, QuEChERS, 关键词 : ; ; ; Research progress of overview on sample pretreatment of pesticides residue in milk LIU Hui-Ling * (Hebei Entry-exit Inspection and Quarantine Bureau, Shijiazhuang , China) ABSTRACT: The level of pesticide residues in milk is relatively quite high as milk is close to the top of food chain. So the harmful substance in milk had attracted much attention of consumer. With the increase of public attention to food safety, detection of pesticide and veterinary drug residues in milk has become a hot topic of food safety in today s China. Meanwhile, sample preparation is a very critical step in the determination process and it determines the analysis accuracy and precision. This article makes a brief summary of liquid-liquid extraction, solid phase extraction, solid phase microextraction, matrix solid-phasedispersion extraction, Gel Permeation Chromatography, cloud point extraction, and QuEChERS. This article reviewed the new research progress of sample preparation of pesticide residues in milk, aimed to supply some reference to the further research in this area. KEY WORDS: milk; pesticide; residues; determination 1 引言 A B, kcal 3.00 g 3.20 g ug A,,, 120, 98,,,,, * 通讯作者 :,, lingling85@aliyun.com *Corresponding author: LIU Hui-Ling, Master, Institute of Food Safety, Technical Center of He Bei Entry-Exit Inspection & Quaran tine Bureau, No.318, Heping Road, Shijiazhuang , China. lingling85@aliyun.com

2 1420 5,, [1-4],,,, , BHC DDT GB α ,,,, 2 牛奶中农药残留的来源 现状及其危害 2.1 牛奶中农药残留的来源,,,, [5],,,,, : 1,, [[6,7] ; 2, [6,7] ; 3,,, [6,7] 2.2 牛奶中农药残留的现状及危害, 10%, 90%,,,,,,,,,,,,, ;,,, [4,8] 3 农药残留检测的研究进展,,,,, 3.1 液液萃取 (LLE), ( ),, [9],,,,,,,, [10] - (1:1, V:V),,

3 5 : 1421,,,,, 3.2 固相萃取 (SPE),,,,,, [11],, [12],,, Florisil [12], C 18, Bordet [13], C 18 Florisil, ; [14] Florisil (GC) ; [15] Florisil / (1/1, v/v), - 19, μg/kg [16], C 18, : 92.5%~95.6% 91.6%~93.4%, 0.4 ng 0.1 ng [18] C 18, ~0.62 μg/l 60.4%~118.4% ; 0.56~2.48 μg/l 64.4%~118.5%,,,, SPE, 3.3 固相微萃取 (SPME),,,, 2 1,,,,,,,,, [19],,, ~0.2 μg/l, 85%~110% González-Rodríguez [15] -GC- (MS/MS),,, 3.4 基质分散固相萃取 (MSPD) Barker 1989 [11,12] Florisil ph,, [21],,,

4 [22], [23] GC-MS/MS 13,,, [24] C 18 Primary Secondary Amine (PSA), - (UPLC-MS /MS), (ESI+) (MRM), 0.01 mg/kg, 62.8%~107%, 4.2%~19%, MSPD,,, 3.5 凝胶渗透色谱 (GPC),,,,, [22,25] GPC [26], 10 ; %~108.86%, 10.88%, 0.042~0.199 μg/kg,, 3.6 浊点萃取 (CPE) -,, [27], ( ),, ( ),,,,, [27], [28-32],, [33,34] [35],, 6, 85.09%~96.74%, 1.90%~3.98% 6 (MRL),,,,, 3.7 QuEChERS 法 QuEChERS [36-38],, [39,40],, ; PSA(N- ),, PSA [41], C 18 QuEChERS,,, [42,43] 昇 [44] QuEChERS,,, 8, 0.001~0.008 mg/kg, 65.09%~100.02%, RSD 2.96%~11.64%, 昇 [44]

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8 Cheap, Effective, Rugged and Safe.) approach [J]. Anal Chimica Acta, 2010, 637(1/2): [48] Koesukwiwat U, Lehotay SJ, Miao S, et al. High throughput analysis of 150 pesticides in fruits and vegetables using QuEChERS and low-pressure gas chromatography-time-of-flight mass spectrometry[j]. J Chromatogr A, 2010, 1217(43): ( 责任编辑 : 邓伟 ) 作者简介 刘慧玲, 硕士, 主要研究方向为食品安全 lingling85@aliyun.com 转基因食品安全 专题征稿 30, 2001 SCI 14 ISO 投稿方式 : tougao@chinafoodj.com 食品安全质量检测学报 编辑部